CN102951693A - Method for processing and recycling production wastewater of fluorescent brightener CBS - Google Patents
Method for processing and recycling production wastewater of fluorescent brightener CBS Download PDFInfo
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- CN102951693A CN102951693A CN2012104747630A CN201210474763A CN102951693A CN 102951693 A CN102951693 A CN 102951693A CN 2012104747630 A CN2012104747630 A CN 2012104747630A CN 201210474763 A CN201210474763 A CN 201210474763A CN 102951693 A CN102951693 A CN 102951693A
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Abstract
The invention relates to a method for processing and recycling production wastewater of a fluorescent brightener CBS, belonging to the technical field of production of the fluorescent brighteners, which comprises the following steps of: processing production wastewater of the CBS by a distillation manner, and recycling fraction and salt slag, wherein the fraction is directly used for a refining process of the production of the CBS, the salt slag is purified by methyl alcohol which is a byproduct of the production of the CBS, and is subjected to solid-liquid separation to obtain refined salt, and the refined salt is directly used for a salting-out process of the production of the CBS. According to the invention, the problem that the production wastewater of the CBS is difficultly processed can be solved, so that the wastewater zero emission of the production of the CBS is realized; the processing method is green and environment-friendly; simultaneously, the methyl alcohol which is the byproduct of the production of the CBS is reasonably utilized, and the salt slag is effectively processed and utilized, so that the raw and auxiliary materials can be recycled; and further, the process is optimized, and the cost is reduced.
Description
Technical field
The invention belongs to the white dyes production technical field, relate to a kind for the treatment of process of fluorescent brightener CBS factory effluent, and the method for being utilized by resource recycling.
Background technology
Fluorescent brightener CBS is a kind of white dyes of excellent performance, have that good anti-chlorine floats, acid and alkali-resistance, sun-resistant performance, mainly be used in washing powder, washing cream, soap, perfumed soap and the liquid washing agent, playing the effect of brightening, increase gorgeous and blast, is one of white dyes kind of effect the best in the detergent industry.
At present, following operational path is mostly adopted in the production of CBS: 1) condensation reaction: with 4,4 ＇-dimethylene bisphosphate diethyl-ester group biphenyl (english abbreviation: BPMB), ortho-sulfonic acid sodium phenyl aldehyde, methyl alcohol-sodium methoxide solution be raw material, with N, N-dimethyl formamide (DMF) or dimethyl sulfoxide (DMSO) (DMSO) are reaction medium, carry out the Witting-Horner condensation reaction; 2) distillation: the distillation reaction mother liquor, reclaim methyl alcohol, DMF or DMSO; 3) saltout: moisturizing in the distilled and concentrated solution, heat up and make it entirely molten, add salt and cooling is separated out product, press filtration gets CBS coarse filtration cake, has produced simultaneously a large amount of CBS waste water; 4) make with extra care: CBS coarse filtration cake adds water and mixes rear making beating, and heating makes it to dissolve, heat filtering, and the rear press filtration of cooling gets the CBS paste, and the refinement mother liquor reuse is as the water of the workshop section of saltouing; 5) drying: the CBS paste obtains work in-process through expansion drying, and reaction principle is as follows:
Can find out from above operational path, the waste water of CBS is from the workshop section of saltouing, and the salts contg in the waste water surpasses 20000mg/L.In order to search out best CBS method of wastewater treatment, present document is retrieved.Confirm most white dyes waste water by retrieval, all adopt materialization and the biochemical treatment process that combines, as follows:
Patent CN200910097913.9, disclose white dyes waste water and passed through first multistage physico-chemical pretreatment, comprise: catalytic reduction dehalogenation, coagulating sedimentation and the catalytic wet oxidation of Fe-C-Cu system, then adopt double oxygen take urethane as carrier and the biological filtering tank process of aerobic combination to process.
Patent CN201010168745.0 discloses a kind of comprehensive treatment method for fluorescent brightener production wastewater: fluorescent brightener production wastewater enters successively equalizing tank, coagulative precipitation tank, hydrolysis acidification pool, Aerobic Pond, ultrasonic degradation device and membrane bioreactor and processes.
Author Wang Jianhang etc. are in the November in 2009 the 35th of " water technology " volume o. 11th, deliver article " processing of fluorescent brightener production wastewater ", introduced the method that adopts " the little electrolysis-acidication of aeration iron charcoal-aerobe processing-ozone oxidation " technique that fluorescent brightener production wastewater is processed.
Author Liu Feifei etc. are in " water supply and drainage " the 01st phase in 2012, delivered article " fluorescent brightener production wastewater processing feasibility study ", introduced and adopt acid out coagulation-acidication-IC reactor-Fenton oxidation-A/O-ozonation technology to the treatment process of fluorescent brightener production wastewater.
To sum up, the treatment process of the white dyes waste water of bibliographical information all is the combined method of wastewater treatment of materialization-biochemistry at present.Do not see after the wastewater treatment again by the report of recycling.But the application limitation of biochemical process is to be only applicable to the wastewater treatment of salts contg below 5000mg/L; When salts contg was higher than 5000mg/L, treatment effect obviously descended, and its cause is the Coal Gas Washing Cycling Water salinity, can suppress the microorganism active in the routine biochemistry treatment process.And the salts contg of CBS waste water exceeds approximately several times of 5000mg/L, if adopt biochemical process to dilute with clear water first, so that can process after the salts contg reduction, but the drawback of this method is to consume water resources, and wastewater flow rate is increased.
Summary of the invention
The present invention be directed to high content of salt fluorescent brightener CBS factory effluent, and a kind of method of processing and recycle of fluorescent brightener CBS factory effluent is provided.
The present invention is achieved by the following technical solutions:
A kind of processing of fluorescent brightener CBS factory effluent and the method for recycle may further comprise the steps:
(1) processing of waste water: adopt the distillation mode that the CBS factory effluent is processed, and reclaim cut and salt slag;
(2) resource recycling utilization: cut directly is used to the refining workshop section that CBS produces; The salt slag utilizes the by-product carbinol in the CBS production to purify, and obtains purified salt through solid-liquid separation again, and this salt directly is used to the workshop section of saltouing that CBS produces.
Further, described distillation mode is air distillation, underpressure distillation or MVR distillation, the MVR distillation that preferred energy consumption is minimum, the MVR system recompresses the steam that produces in the evaporative process, steam recirculation after compression is used as the thermal medium of distillation, greatly improve the utilization ratio of steam, the energy consumption cost of distillation is far below multiple-effect evaporator.
Described salt slag contains organic impurity, can not directly utilize.This salt slag utilizes CBS to produce the by-product methyl alcohol of distillation workshop section, purifies, and the mass ratio of salt slag and methyl alcohol is 1:1 ~ 5; Obtain purified salt and useless methyl alcohol through solid-liquid separation.The useless methyl alcohol that produces after the salt slag is purified obtains industrial grade benzenemethanol by rectifying, and the remaining organic detritus in rectifying still bottom burns by boiler.Again, described cut is colourless transparent liquid, COD
CrValue can not directly be discharged generally at 10000 mg/L-20000mg/L; If process by materialization and biochemical mode, cost is higher; The present invention proposes the refining workshop section of cut direct reuse to CBS production, and does not affect the CBS quality product.
Compared with prior art, the present invention has the following advantages:
(1) for biochemical process the high-salt wastewater that can not directly process, the invention provides that a kind of effect is excellent, cost is low and can realize industrialized treatment process;
(2) the present invention has rationally utilized the distillation of CBS waste water to process the cut that produces, and is used to the refining workshop section that CBS produces, and has realized the recycle of resource.
(3) the present invention has rationally utilized the by-product methyl alcohol in the CBS production, and the CBS waste water that is used for purifying distills the salt slag that produces in the processing, and the workshop section of saltouing that the purified salt after the purification is used in CBS has realized the recycle of resource.
(4) technical process of the present invention is simple, and processing cost is low.
Description of drawings
Fig. 1 is FB(flow block) of the present invention.
Embodiment
Embodiment 1
Test one: get normal batch CBS factory effluent 5000 grams, and place four-hole boiling flask, adopt air distillation, collect cut in the still-process, after distillation finishes, obtain cut 4875 grams, salt slag 125 grams.
The salt slag is dropped in the four-hole boiling flask of 1000ml, add the 500 gram by-product methyl alcohol of producing distillation workshop section from CBS, stirred 30 minutes, the salt slag is scattered in the methyl alcohol fully, Büchner funnel filters and obtains purified salt 110 grams and useless methyl alcohol 515 grams.Useless methyl alcohol obtains methyl alcohol 480 grams after rectifying, organic detritus 35 grams.
The methyl alcohol that rectifying obtains is through gas chromatographic detection, content 99.2%.
Test two: will test CBS synthetic that a cut that reclaims and purified salt are used for the laboratory, the CBS product that obtains is 1#, and the Salting-Out Waste Water that experiment obtains continues to process by the method for testing one.Technical process as shown in Figure 1.
Test three is to test six: according to test two method, the cut that experiment is obtained and purified salt recycling 4 times obtain respectively 2#, 3#, 4#, 5#CBS product.According to the industry standard HG/T3726-2010 of fluorescent brightener CBS, detect five CBS sample qualities of gained, comprising: outward appearance, smell, maximum absorption wavelength, uv-absorbing and moisture.
| Numbering | Outward appearance | Smell | Maximum absorption wavelength/nm | Uv-absorbing | Moisture/% |
| 1# | The yellow-green colour uniform powder | Tasteless | 349.0 | 1244 | 0.9 |
| 2# | The yellow-green colour uniform powder | Tasteless | 349.4 | 1238 | 1.1 |
| 3# | The yellow-green colour uniform powder | Tasteless | 349.7 | 1236 | 1.4 |
| 4# | The yellow-green colour uniform powder | Tasteless | 349.0 | 1240 | 1.0 |
| 5# | The yellow-green colour uniform powder | Tasteless | 349.1 | 1239 | 1.2 |
| 6# | The yellow-green colour uniform powder | Tasteless | 348.9 | 1239 | 1.2 |
Following table has been listed above-mentioned after continuous 5 recycles, the statistic of attribute data of the CBS product (being numbered 6#) of resulting CBS product (being numbered 1#, 2#, 3#, 4#, 5#) and the normal production batch in workshop.
As can be seen from the above table: along with the increase of the recycle number of times that reclaims cut and salt, the CBS quality product finds no downward trend, and treatment process does not affect the quality of CBS.
Embodiment 2
Adopt MVR system (configuration U.S. Thailand knows the vapour compressor of your company's production and adopts the forced circulation evaporation crystallizer), distill 2000 kilograms of CBS factory effluents, reclaim cut 1950Kg, the residual salts slag is 50 kilograms in the vaporizer.
In 1 cube enamel still, add CBS and produce 200 kilograms of distillation workshop section recovery by-product methyl alcohol, open and stir, then 50 kilograms of salt slags are put in the still, stirred 30 minutes, the salt slag is well-dispersed in the methyl alcohol, press filtration obtains 44 kilograms of purified salts, 206 kilograms of useless methyl alcohol, useless methyl alcohol obtains 192 kilograms of methyl alcohol, 14 kilograms of organic detritus after rectifying.
The methyl alcohol that rectifying obtains is through gas chromatographic detection, content 99.3%.
Adopt the MVR system to process waste water, the power consumption cost is about 45 yuan/tons.
Embodiment 3
Adopt air distillation that 2000 kilograms CBS waste water is processed, other operation is with embodiment 2.Waste water is processed in air distillation, and the power consumption cost is about 300 yuan/tons.
Embodiment 4
Adopt underpressure distillation that 2000 kilograms CBS waste water is processed, vacuum tightness is at 0.5Kg/cm
3, other operation is with embodiment 2.Waste water is processed in underpressure distillation, and the power consumption cost is about 180 yuan/tons.
Embodiment 5
A kind of processing of fluorescent brightener CBS factory effluent and the method for recycle may further comprise the steps:
(1) processing of waste water: adopt MVR distillation mode that the CBS factory effluent is processed, and reclaim cut and salt slag;
(2) resource recycling utilization: cut directly is used to the refining workshop section that CBS produces; The salt slag utilizes the by-product carbinol in the CBS production to purify, and the mass ratio of salt slag and methyl alcohol is 1:1, obtains purified salt through solid-liquid separation again, and this salt directly is used to the workshop section of saltouing that CBS produces.
The CBS product that finally obtains is through suitable to the quality of the 6# sample among its indices detection and the embodiment 1.
Embodiment 6
A kind of processing of fluorescent brightener CBS factory effluent and the method for recycle may further comprise the steps:
(1) processing of waste water: adopt MVR distillation mode that the CBS factory effluent is processed, and reclaim cut and salt slag;
(2) resource recycling utilization: cut directly is used to the refining workshop section that CBS produces; The salt slag utilizes the by-product carbinol in the CBS production to purify, and the mass ratio of salt slag and methyl alcohol is 1:5, obtains purified salt through solid-liquid separation again, and this salt directly is used to the workshop section of saltouing that CBS produces.
The CBS product that finally obtains is through suitable to the quality of the 6# sample among its indices detection and the embodiment 1.
Embodiment 7
A kind of processing of fluorescent brightener CBS factory effluent and the method for recycle may further comprise the steps:
(1) processing of waste water: adopt MVR distillation mode that the CBS factory effluent is processed, and reclaim cut and salt slag;
(2) resource recycling utilization: cut directly is used to the refining workshop section that CBS produces; The salt slag utilizes the by-product carbinol in the CBS production to purify, and the mass ratio of salt slag and methyl alcohol is 1:3, obtains purified salt through solid-liquid separation again, and this salt directly is used to the workshop section of saltouing that CBS produces.
The CBS product that finally obtains is through suitable to the quality of the 6# sample among its indices detection and the embodiment 1.
Claims (4)
1. the method for the processing of a fluorescent brightener CBS factory effluent and recycle is characterized in that, may further comprise the steps:
1) processing of waste water: adopt the distillation mode that the CBS factory effluent is processed, and reclaim cut and salt slag;
2) resource recycling utilization: cut directly is used to the refining workshop section that CBS produces; The salt slag utilizes the by-product carbinol in the CBS production to purify, and obtains purified salt through solid-liquid separation again, and this salt directly is used to the workshop section of saltouing that CBS produces.
2. the method for the processing of fluorescent brightener CBS factory effluent according to claim 1 and recycle is characterized in that, described distillation mode is air distillation, underpressure distillation or MVR distillation, the MVR distillation that preferred energy consumption is minimum.
3. the method for the processing of fluorescent brightener CBS factory effluent according to claim 1 and 2 and recycle is characterized in that, when described salt slag was purified, the salt slag mixed 1:1 ~ 5 in mass ratio with by-product methyl alcohol.
4. the method for the processing of fluorescent brightener CBS factory effluent according to claim 3 and recycle is characterized in that, the useless methyl alcohol that produces after the salt slag is purified obtains industrial grade benzenemethanol by rectifying, and the remaining organic detritus in rectifying still bottom burns by boiler.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408196A (en) * | 2013-08-21 | 2013-11-27 | 山西青山化工有限公司 | Method for treating wastewater containing fluorescent whitening agent |
| CN103420543A (en) * | 2013-08-13 | 2013-12-04 | 山西青山化工有限公司 | Processing method of production waste water containing sulfo fluorescent whitening agent |
| CN103435222A (en) * | 2013-08-21 | 2013-12-11 | 山西青山化工有限公司 | Method for treating flourescent brightener wastewater with phosphorus |
| CN106008284A (en) * | 2016-06-21 | 2016-10-12 | 太仓市东明化工有限公司 | Wastewater treatment method for fluorescent whitening agent CBW |
| CN106517627A (en) * | 2016-11-30 | 2017-03-22 | 安徽普朗膜技术有限公司 | Fluorescent whitening agent production wastewater treatment system |
| CN113562894A (en) * | 2021-08-20 | 2021-10-29 | 桂林南药股份有限公司 | Treatment method and treatment system for DMF (dimethyl formamide) wastewater and DMSO (dimethyl sulfoxide) wastewater |
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| CN103420543A (en) * | 2013-08-13 | 2013-12-04 | 山西青山化工有限公司 | Processing method of production waste water containing sulfo fluorescent whitening agent |
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| CN106008284A (en) * | 2016-06-21 | 2016-10-12 | 太仓市东明化工有限公司 | Wastewater treatment method for fluorescent whitening agent CBW |
| CN106517627A (en) * | 2016-11-30 | 2017-03-22 | 安徽普朗膜技术有限公司 | Fluorescent whitening agent production wastewater treatment system |
| CN113562894A (en) * | 2021-08-20 | 2021-10-29 | 桂林南药股份有限公司 | Treatment method and treatment system for DMF (dimethyl formamide) wastewater and DMSO (dimethyl sulfoxide) wastewater |
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